Cyclopropylmethylsulphinic acid → HCID 22054098, 화합물

HRID 1796134

반응식

HRID 1796134 반응식
[CH:1]1([CH2:4][S:5]([OH:7])=[O:6])[CH2:3][CH2:2]1.[CH2:8]=[C:9]([CH2:13][C:14]([N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1)=[O:15])[C:10]([OH:12])=[O:11]>C1(C)C=CC=CC=1.C(#N)C>[CH:1]1([CH2:4][S:5]([CH2:8][CH:9]([CH2:13][C:14]([N:16]2[CH2:17][CH2:18][O:19][CH2:20][CH2:21]2)=[O:15])[C:10]([OH:12])=[O:11])(=[O:7])=[O:6])[CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 17937320Cyclopropylmethylsulphinic acidHCID 220540222-Methylene4-morpholin-4-yl-4-oxo-butyric acid

생성물 1

HCID 22054098HCID 22054098, 화합물수율 40.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6342Acetonitrile용매

반응 조건

온도
85 °C

실험 절차

To a solution of cyclopropylmethylsulphinic acid (1.8 g, 15 mmol) in anhydrous toluene (45 mL) and anhydrous acetonitrile (9 mL) was added 2-Methylene4-morpholin-4-yl-4-oxo-butyric acid (2.98 g, 15 mmol). The resulting solution was warmed to 85° C. and stirred at this temperature for 4.5 h. The heterogeneous reaction mixture is then allowed to cool to room temperature then concentrated under reduced pressure. The residue is then purified by flash chromatography eluting with 7% methanol in dichloromethane to give 2-Cyclopropylmethanesulfonylmethyl-4-morpholin-4-yl-4-oxo-butyric acid (1.92 g) as viscous oil which was re crystallized from hot ethyl acetate to give a white solid.

후처리

  1. temperatureto cool to room temperature
  2. concentrationthen concentrated under reduced pressure
  3. customThe residue is then purified by flash chromatography
  4. washeluting with 7% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-eeb3f2e7ab404a5f96dc1a8bc5ff6cc1
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07030116B2

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